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Crystal structure of di-μ-chloro-acetato-hexa-kis-(di-methyl-formamide)-tetra-kis-(μ-N,2-dioxido-benzene-1-carboximidato)tetra-manganese(III)disodium dimethyl-formamide disolvate.

Daly CI, Zeller M, Zaleski CM - Acta Crystallogr Sect E Struct Rep Online (2014)

Bottom Line: The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hydroximate, and DMF is N,N-di-methyl-formamide, is reported.Weak C-H⋯O inter-actions, in addition to pure van der Waals forces, contribute to the overall packing of the mol-ecules.The solvent molecule is also disordered over two sets of sites, with an occupancy ratio of 0.615 (5):0.385 (5).

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry, Shippensburg University, 1871 Old Main Dr., Shippensburg, PA 17257, USA.

ABSTRACT
The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hydroximate, and DMF is N,N-di-methyl-formamide, is reported. The macrocyclic metallacrown consists of an -[Mn(III)-N-O]4- ring repeat unit and the metallacrown captures two Na(+) ions in the central cavity above and below the plane of the metallacrown. Each Na(+) ion is seven-coordinate and is bridged to two ring Mn(III) ions, through either a coordinating DMF mol-ecule or a chloro-acetate anion. The ring Mn(III) ions have either a tetra-gonally distorted octa-hedral geometry or a distorted square-pyramidal geometry. Weak C-H⋯O inter-actions, in addition to pure van der Waals forces, contribute to the overall packing of the mol-ecules. The complete molecule has inversion symmetry and is disordered over two sets of sites with an occupancy ratio of 0.8783 (7):0.1217 (7). The solvent molecule is also disordered over two sets of sites, with an occupancy ratio of 0.615 (5):0.385 (5).

No MeSH data available.


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Molecular structure of Na2(O2CCH2Cl)2[12-MCMnIIIN(shi)-4](DMF)6·2DMF (side view). The stepped or ruffled character of the structure is emphasised in this view. Atom labels for all non-hydrogen atoms of the axial DMF and chloro­acetate ligands on one asymmetric unit have been provided. See Fig. 1 ▶ for display details.
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fig2: Molecular structure of Na2(O2CCH2Cl)2[12-MCMnIIIN(shi)-4](DMF)6·2DMF (side view). The stepped or ruffled character of the structure is emphasised in this view. Atom labels for all non-hydrogen atoms of the axial DMF and chloro­acetate ligands on one asymmetric unit have been provided. See Fig. 1 ▶ for display details.

Mentions: The title compound consists of the typical 12-MCMnIIIN(shi)-4 framework with four MnIII—N—O repeating units producing an overall square-geometry mol­ecule (Fig. 1 ▶). As in other di-sodium 12-MCMnIIIN(shi)-4 complexes (Lah & Pecoraro, 1991 ▶; Gibney et al., 1996 ▶; Kessissoglou et al., 2002 ▶; Azar et al., 2014 ▶), an inversion center is located in the central MC cavity produced by the oxime oxygen atoms of the shi3− ligands. In addition, two Na+ ions are captured in the central cavity on opposite faces of the MC (Fig. 2 ▶). A chloro­acetate anion bridges each Na+ ion to a ring manganese ion. The entire mol­ecule (metallacrown, chloro­acetate counter-anions, and coordinating DMF mol­ecules) is disordered over two sites with an occupancy ratio of 0.8783 (7):0.1217 (7) (complete refinement details are given below); thus, a description will only be given for the higher occupancy component. The metallacrown is nearly planar, but it can be considered to possess a stepped structure, i.e. the MC is ruffled (Fig. 2 ▶). Charge neutrality is maintained for the mol­ecule by the presence of four MnIII and two Na+ cations and four shi3− and two chloro­acetate anions. The oxidation state assignment of the ring MnIII ions is supported by the average bond lengths, bond-valence-sum (BVS) calculations, and the presence of elongated axial bond lengths expected for a high-spin d4 electron configuration (Liu & Thorp, 1993 ▶). For Mn1, the average bond length is 2.05 Å and the BVS value is 3.06 valence units (v.u.), and for Mn2 the average bond length is 1.96 Å and the BVS value is 2.98  v.u.


Crystal structure of di-μ-chloro-acetato-hexa-kis-(di-methyl-formamide)-tetra-kis-(μ-N,2-dioxido-benzene-1-carboximidato)tetra-manganese(III)disodium dimethyl-formamide disolvate.

Daly CI, Zeller M, Zaleski CM - Acta Crystallogr Sect E Struct Rep Online (2014)

Molecular structure of Na2(O2CCH2Cl)2[12-MCMnIIIN(shi)-4](DMF)6·2DMF (side view). The stepped or ruffled character of the structure is emphasised in this view. Atom labels for all non-hydrogen atoms of the axial DMF and chloro­acetate ligands on one asymmetric unit have been provided. See Fig. 1 ▶ for display details.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4257439&req=5

fig2: Molecular structure of Na2(O2CCH2Cl)2[12-MCMnIIIN(shi)-4](DMF)6·2DMF (side view). The stepped or ruffled character of the structure is emphasised in this view. Atom labels for all non-hydrogen atoms of the axial DMF and chloro­acetate ligands on one asymmetric unit have been provided. See Fig. 1 ▶ for display details.
Mentions: The title compound consists of the typical 12-MCMnIIIN(shi)-4 framework with four MnIII—N—O repeating units producing an overall square-geometry mol­ecule (Fig. 1 ▶). As in other di-sodium 12-MCMnIIIN(shi)-4 complexes (Lah & Pecoraro, 1991 ▶; Gibney et al., 1996 ▶; Kessissoglou et al., 2002 ▶; Azar et al., 2014 ▶), an inversion center is located in the central MC cavity produced by the oxime oxygen atoms of the shi3− ligands. In addition, two Na+ ions are captured in the central cavity on opposite faces of the MC (Fig. 2 ▶). A chloro­acetate anion bridges each Na+ ion to a ring manganese ion. The entire mol­ecule (metallacrown, chloro­acetate counter-anions, and coordinating DMF mol­ecules) is disordered over two sites with an occupancy ratio of 0.8783 (7):0.1217 (7) (complete refinement details are given below); thus, a description will only be given for the higher occupancy component. The metallacrown is nearly planar, but it can be considered to possess a stepped structure, i.e. the MC is ruffled (Fig. 2 ▶). Charge neutrality is maintained for the mol­ecule by the presence of four MnIII and two Na+ cations and four shi3− and two chloro­acetate anions. The oxidation state assignment of the ring MnIII ions is supported by the average bond lengths, bond-valence-sum (BVS) calculations, and the presence of elongated axial bond lengths expected for a high-spin d4 electron configuration (Liu & Thorp, 1993 ▶). For Mn1, the average bond length is 2.05 Å and the BVS value is 3.06 valence units (v.u.), and for Mn2 the average bond length is 1.96 Å and the BVS value is 2.98  v.u.

Bottom Line: The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hydroximate, and DMF is N,N-di-methyl-formamide, is reported.Weak C-H⋯O inter-actions, in addition to pure van der Waals forces, contribute to the overall packing of the mol-ecules.The solvent molecule is also disordered over two sets of sites, with an occupancy ratio of 0.615 (5):0.385 (5).

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry, Shippensburg University, 1871 Old Main Dr., Shippensburg, PA 17257, USA.

ABSTRACT
The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hydroximate, and DMF is N,N-di-methyl-formamide, is reported. The macrocyclic metallacrown consists of an -[Mn(III)-N-O]4- ring repeat unit and the metallacrown captures two Na(+) ions in the central cavity above and below the plane of the metallacrown. Each Na(+) ion is seven-coordinate and is bridged to two ring Mn(III) ions, through either a coordinating DMF mol-ecule or a chloro-acetate anion. The ring Mn(III) ions have either a tetra-gonally distorted octa-hedral geometry or a distorted square-pyramidal geometry. Weak C-H⋯O inter-actions, in addition to pure van der Waals forces, contribute to the overall packing of the mol-ecules. The complete molecule has inversion symmetry and is disordered over two sets of sites with an occupancy ratio of 0.8783 (7):0.1217 (7). The solvent molecule is also disordered over two sets of sites, with an occupancy ratio of 0.615 (5):0.385 (5).

No MeSH data available.


Related in: MedlinePlus