Synthesis and Crystal Structure of MnII(OAc)2[15-MC Mn III (N)shi-5](Im)3(EtOH)3 (shi3− = salicylhydroximate, −OAc = acetate, Im = imidazole, and EtOH = ethanol)

Emerich, Brian; Smith, Matthew J.; Zeller, Mat­thias; Zaleski, Curtis M.

doi:10.1007/s10870-010-9735-5

Cited by 10 publications

(6 citation statements)

References 19 publications

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“…For related manganese and vanadium metallacrown structures, see: Lah & Pecoraro (1989) and , respectively. For related Mn(II)[15-MC Mn(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 (2011Tigyer et al ( , 2012. For an explanation on how to calculate the s/h ratio, see: Stiefel & Brown (1972).…”

Section: Related Literaturementioning

confidence: 99%

μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

Tigyer¹,

Zeller²,

Zaleski³

2013

Acta Cryst E

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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 Λ 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)].

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Section: Related Literaturementioning

confidence: 99%

μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

Tigyer¹,

Zeller²,

Zaleski³

2013

Acta Cryst E

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“…For a general review of metallacrowns, see: Mezei et al (2007). For related Mn(II)[15-MC Mn(III)N(shi) -5)] structures and related synthetic procedures, see: Kessissoglou et al (1994); Dendrinou-Samara et al (2001, 2002, 2005; Emerich et al (2010); Tigyer et al (2011). For an explanation on how to calculate , see: Addison et al (1984).…”

Section: Related Literaturementioning

confidence: 99%

“…The family of manganese-based 15-MC-5 complexes, which consists of a 15 membered ring with a -[Mn(III)-N-O] 5 -repeat unit and a central Mn(II) ion, have shown better antibacterial activity than simple manganese-herbicide complexes (Dendrinou-Samara et al, 2002, 2005). The first few Mn-based 15-MC-5 complexes were made with pyridine molecules bound to the structure (Kessissoglou et al, 1994;Dendrinou-Samara et al, 2001, 2002, 2005; however, it has recently been shown that imidazole can also be used to produce a Mn-based 15-MC-5 complex (Emerich et al, 2010;Tigyer et al 2011).…”

Section: Data Collectionmentioning

confidence: 99%

“…3 d-e). In previous Mn(II)[15-MC Mn(III) -5] structures, the coordination spheres of the Mn ions had been completed by forming bonds to the oxygen atoms of the carboxylate anions (Kessissoglou et al, 1994;Dendrinou-Samara et al, 2001, 2002, 2005Emerich et al, 2010;and Tigyer et al, 2011); however, in 1 these bonds do not exist. The geometry about Mn2, Mn5, and Mn6 is best described as a distorted octahedron (Fig.…”

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confidence: 99%

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Pentakis(μ₃-N,2-dioxidobenzene-1-carboximidato)di-μ₂-formato-pentakis(1H-imidazole)methanolpentamanganese(III)manganese(II)–methanol–water (1/3.36/0.65)

2012

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Key indicators: single-crystal X-ray study; T = 100 K; mean (C-C) = 0.005 Å; disorder in main residue; R factor = 0.049; wR factor = 0.140; data-to-parameter ratio = 17.5.The title compound, [Mn 6 (C 7 with a geometry best described as between facecapped trigonal-prismatic and face-capped octahedral. Three Mn III ions of the metallacrown ring are six-coordinate with distorted octahedral geometries. Of these six-coordinate Mn III ions, two have mirror-plane configurations, while the other has a Á absolute stereoconfiguration. The remaining two Mn III ions have a coordination number of five with a distorted square-pyramidal geometry. The five imidazole ligands are bound to five different Mn III ions. Disorder is observed for one of the coordinating imidazole ligands, as the imidazole ligand is disordered over two alternative mutually exclusive positions in a ratio of 0.672 (9) to 0.328 (9). The interstitial voids between the main molecules that constitute the structure are mostly filled with methanol molecules that form hydrogenbonded chains. Some of the sites of the non-coordinated methanol molecules are not fully occupied, with the remainder of the volume either empty or taken up by ill-defined close to amorphous content. One site was refined as being taken up by either two or one methanol molecules, with an occupancy ratio of 0.628 (5) to 0.343 (5). This disorder might thus be correlated with the disorder of the imidazole ring (an N-HÁ Á ÁO hydrogen bond between the major moieties of the imidazole and the methanol molecules is observed). On the other side of the disordered imidazole ring the chain of partially occupied methanol molecules originates that extends via O-HÁ Á ÁO hydrogen bonds to the metal-coordinated methanol molecule. The three partially occupied methanol molecules were refined to be disordered with two water molecules to take two residual electron density peaks into account (the exact nature of these weak residual electron density peaks cannot be deduced from the X-ray diffraction data alone, the assignment as water is tentative). The occupancy rate for the methanol molecules refined to 0.480 (7). The occupancy rate of the two water molecules refined to 0.34 (1) and 0.31 (2) for each site. Related literature ExperimentalCrystal data H atoms treated by a mixture of independent and constrained refinement Á max = 2.17 e Å À3 Á min = À0.59 e Å À3 metal-organic compounds

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“…Associated with the minor component is a partially occupied water molecule [total occupancy 0.124 (15)]. structures, see: Kessissoglou et al (1994); Dendrinou-Samara et al (2002, 2005; Emerich et al (2010). For an explanation of how to calculate the s/h ratio, see: Stiefel & Brown (1972).…”

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Di-μ-acetato-bis(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)tetrakis(1-ethylimidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylforamide–methanol–water (1/1/1/1/0.12)

2011

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Synthesis and Crystal Structure of MnII(OAc)2[15-MC Mn III (N)shi-5](Im)3(EtOH)3 (shi3− = salicylhydroximate, −OAc = acetate, Im = imidazole, and EtOH = ethanol)

Cited by 10 publications

References 19 publications

μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

Pentakis(μ₃-N,2-dioxidobenzene-1-carboximidato)di-μ₂-formato-pentakis(1H-imidazole)methanolpentamanganese(III)manganese(II)–methanol–water (1/3.36/0.65)

Di-μ-acetato-bis(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)tetrakis(1-ethylimidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylforamide–methanol–water (1/1/1/1/0.12)

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Synthesis and Crystal Structure of MnII(OAc)2[15-MC Mn III (N)shi-5](Im)3(EtOH)3 (shi3− = salicylhydroximate, −OAc = acetate, Im = imidazole, and EtOH = ethanol)

Cited by 10 publications

References 19 publications

μ3-Acetato-μ2-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

μ3-Acetato-μ2-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

Pentakis(μ3-N,2-dioxidobenzene-1-carboximidato)di-μ2-formato-pentakis(1H-imidazole)methanolpentamanganese(III)manganese(II)–methanol–water (1/3.36/0.65)

Di-μ-acetato-bis(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)tetrakis(1-ethylimidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylforamide–methanol–water (1/1/1/1/0.12)

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μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

μ₃-Acetato-μ₂-acetato-(dimethylformamide)pentakis(μ-N,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1H-imidazole)pentamanganese(III)manganese(II)–diethyl ether–dimethylformamide–methanol–water (1/1/1/1/0.49)

Pentakis(μ₃-N,2-dioxidobenzene-1-carboximidato)di-μ₂-formato-pentakis(1H-imidazole)methanolpentamanganese(III)manganese(II)–methanol–water (1/3.36/0.65)