Aqua­azido­{2,2′-[o-phenylenebis(nitrilo­methyl­idyne)]diphenolato}manganese(III) hemihydrate

Xiutang Zhang; Peihai Wei; Bin Li; Chunyong Wu; Bo Hu

doi:10.1107/S1600536809020200

. 2009 Jun 6;65(Pt 7):m707. doi: 10.1107/S1600536809020200

Aquaazido{2,2′-[o-phenylenebis(nitrilomethylidyne)]diphenolato}manganese(III) hemihydrate

Xiutang Zhang ^a,^b,^*, Peihai Wei ^a, Bin Li ^a, Chunyong Wu ^c, Bo Hu ^a

PMCID: PMC2969293 PMID: 21582653

Abstract

In the title compound, [Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O, the Mn^III ion is chelated by the N,N′,O,O′-tetradentate Schiff base ligand and further coordinated by one azide ion and one water molecule in trans positions, resulting in a distorted fac-MnN₃O₃ octahedral arrangement. The O atom of the uncoordinated water molecule lies on a crystallographic twofold axis. In the crystal, O—H⋯O and O—H⋯N hydrogen bonds help to establish the packing.

Related literature

For background to salicylaldehyde complexes, see: Alam et al. (2003 ▶); Zelewsky & von Knof (1999 ▶).

Experimental

Crystal data

[Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O
M _r = 438.33
Monoclinic,
a = 25.100 (10) Å
b = 11.478 (5) Å
c = 12.599 (5) Å
β = 94.175 (3)°
V = 3620 (3) Å³
Z = 8
Mo Kα radiation
μ = 0.77 mm⁻¹
T = 293 K
0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T _min = 0.914, T _max = 0.941
11927 measured reflections
3162 independent reflections
2371 reflections with I > 2σ(I)
R _int = 0.082

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.086
S = 1.00
3162 reflections
280 parameters
4 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.32 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2004 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809020200/hb2977sup1.cif

e-65-0m707-sup1.cif^{(20.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809020200/hb2977Isup2.hkl

e-65-0m707-Isup2.hkl^{(155.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Mn1—O1	1.8636 (18)
Mn1—O2	1.8844 (18)
Mn1—N2	1.986 (2)
Mn1—N1	1.988 (2)
Mn1—N3	2.306 (2)
Mn1—O1W	2.321 (2)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W⋯N3ⁱ	0.82 (2)	2.12 (2)	2.937 (3)	176 (3)
O1W—H1W⋯O2ⁱⁱ	0.820 (11)	2.076 (6)	2.885 (3)	169 (2)
O2W—H3W⋯N5	0.82 (3)	2.18 (3)	3.000 (3)	173 (4)

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

The authors thank the National Ministry of Science and Technology of China (grant No. 2001CB6105–07) for support.

supplementary crystallographic information

Comment

The synthesis of complexes consisting of salicylaldehyde ligand has attracted continuous research interest not only because of their appealing structural and topological novelty, but also due to their unusual optical, electronic, magnetic, and catalytic properties, as well as their potential medical application (Alam et al., 2003; Zelewsky & von Knof, 1999). In the present paper, we describe the synthesis and structural characterizations of the title compound, (I),

As shown in Fig. 1, each Mn(III) atom is chelated by Schiff base ligand via two N and two O atoms and is additionally coordinated by one azide and a water molecule, forming a distorted octahedral geometry (Table 1) in which, the Schiff base lies in the equatorial plane, and the azide and aqua ligands lie in the axial coordination sites.

With O—H···O and O—H···N hydrogen bonds (Table 2), a three-dimensional network is formed as shown in Fig. 2.

Experimental

A mixture of manganese(III) acetylacetonate (1 mmol) and N,N'-bis(2-hydroxy-5-bromobenzyl)1,2-diaminopropane (1 mmol), and dipotassium nickel tetracyanide (1 mmol) in 20 ml methanol was refluxed for several hours. The above cooled solution was filtered and the filtrate was kept in an ice box. One week later, brown blocks of (I) were obtained with a yield of 5%. Anal. Calc. for C₄₀H₃₄Mn₂N₁₀O₇: C 54.75, H 3.88, N 15.97%; Found: C 54.71, H 3.75, N 15.82.